建立了QuEChERS/超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap HRMS)同时检测水产及水产加工品中16种苯并咪唑类和13种硝基咪唑类药物残留的分析方法.样品经乙酸乙酯提取,浓缩近干,用30％(体积分数)甲醇-水溶液定容,乙腈饱和正己烷、氨基(NH2)吸附剂和MgSO4净化.采用Thermo fisher Accucore RP-MS色谱柱(100 mm×2.1 mm,2.6 μm),以0.1％(体积分数)甲酸-乙腈为流动相进行梯度洗脱,使用可加热电喷雾离子源(HESI),全扫描/数据依赖二级扫描(Full MS/dd-MS2,TopN=1)模式检测,外标法定量.结果表明,29种药物在0.5～400 μg/L范围内线性关系良好(r2≥0.9967),在5种水产及水产加工品基质中进行3个不同水平的加标实验,平均回收率为60.2％ ～123.3％,相对标准偏差(n=6)为0.1％～21.7％,方法的定量下限为0.5 ～ 5.0μg/kg.该法操作简便、精密度高、准确性好,适用于批量水产及水产加工品中29种药物的快速检测.%A method was developed for the simultaneous determination of 16 benzimidazoles and 13 nitroimidazoles residues in fish and fishery products using ultrahigh performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry (UPLC-Q-Orbitrap HRMS).The samples were extracted with ethyl acetate,then concentrated and dissolved with 30％methanol aqueous solution,and cleaned up using hexane saturated with acetonitrile,amine (NH2)sorbent and MgSO4.The separation was performed on a Thermo fisher Accucore RP-MS(100 mm ×2.1 mm,2.6 μm) column using acetonitrile and 0.1％ formic acid as mobile phase by gradient elution.The analytes were analyzed in Full MS/dd-MS2 (TopN =1) mode with a heated electrospray ion source (HESI),and quantified by the external standard method.The calibration curves for the 29 analytes were linear in the range of 0.5-400 μg/L with correlation coefficients not less than 0.996 7.The average recoveries at three spiked levels in 5 kinds of product matrixes ranged from 60.2％ to 123.3％ with relative standard deviations(RSDs,n =6) of 0.1％-21.7％.The limits of quantitation were 0.5-5.0 μg/kg.With the advantages of simplicity,high precision and good accuracy,the method is suitable for the rapid detection of 29 veterinary drug residues in aquatic products.
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